自组装管尖固相萃取/超高效液相色谱-高分辨质谱法测定水果中的15种酸性农药

建立自组装管尖固相萃取结合超高效液相色谱-高分辨质谱检测水果中15种酸性农药残留的分析方法。水果样品经甲酸-乙腈(1∶99,体积比)提取后,以官能化聚苯乙烯/二乙烯苯(PEP)和亲水作用色谱(HILIC)作为吸附填料进行管尖固相萃取净化。以T3色谱柱进行色谱分离,采用高分辨质谱的t SIM/dd MS2扫描模式进行定性、定量分析,内标法测定。15种酸性农药在各自线性范围内呈良好的线性关系,相关系数(r2)均大于0.99。方法的定量下限(LOQ)为0.2~10μg/kg。在LOQ,10μg/kg,100μg/kg加标水平下,15种酸性农药的回收率为73.5%~115.9%,相对标准偏差为1.0%~8.3%。该方法灵敏、准确,适用于水果中酸性农药残留的分析测定,具有很好的实际应用价值。

Determination of 15 Acidic Pesticides in Fruit by Ultra High Performance Liquid Chromatography-High Resolution Mass Spectrometry with a Self-assembly Pipette Tip Solid-phase Extraction

A self-assembly pipette tip solid-phase extraction (PTSPE)/high-resolution benchtop Q Exactive mass spectrometric(HRMS) method for the analysis of 15 acidic pesticides in fruit was established.The samples were first extracted with 1％ formic acid in acetonitrile,and then the extracts were cleaned up using PTSPE procedure with the adsorbent of PEP and HILIC.The chromatographic analysis was performed on a T3 column.And the qualitative and quantitative analyses were performed under tSIM/ddMS2 mode by high resolution mass spectrometry.The internal standard calibration was used for quantification,and the method showed a good linearity (r2 ＞ 0.99) in a certain concentration range for the 15 acidic pesticides.The limits of quantitation(LOQ) were between 0.2 μg/kg and 10 μg/kg.The recoveries of the analytes in apples,cherry tomatoes and strawberries samples at spiked levels of LOQ,10 μg/kg and 100 μg/kg ranged from 73.5％ to 115.9％,with relative standard deviations(RSDs) of 1.0％-8.3％.The results showed that the method was sensitive and accurate,and was suitable for the analysis of acidic pesticides in fruit.